CN110312819A - Cylinder type sputtering target and its manufacturing method - Google Patents

Cylinder type sputtering target and its manufacturing method Download PDF

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Publication number
CN110312819A
CN110312819A CN201880011845.7A CN201880011845A CN110312819A CN 110312819 A CN110312819 A CN 110312819A CN 201880011845 A CN201880011845 A CN 201880011845A CN 110312819 A CN110312819 A CN 110312819A
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Prior art keywords
cylinder type
target
sputtering target
raw material
material powder
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CN201880011845.7A
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CN110312819B (en
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鹤田好孝
根岸智哉
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
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    • C04B35/453Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
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    • H01J37/3488Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491Manufacturing of targets
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

Cylinder type sputtering target of the invention has metal cylinder type substrate and cylinder type target made of ceramics, the cylinder type target made of ceramics is engaged with the peripheral side of the cylinder type substrate, integrally formed with the length of the axis direction of 750mm or more, the coefficient of variation of the axis direction of the volume resistivity of the outer peripheral surface of the cylinder type target is 0.05 or less.

Description

Cylinder type sputtering target and its manufacturing method
Technical field
The present invention relates to a kind of cylinder type sputtering target and its manufacturing method, the cylinder type sputtering target has metal circle Cartridge type substrate and cylinder type target made of ceramics, the cylinder type target made of ceramics the peripheral side of the cylinder type substrate with The length of the axis direction of 750mm or more is integrally formed, especially proposes following technology: being able to suppress and molding long size Cylinder type target when the bending that may occur or warpage and seek the homogenization of the target characteristic on axis direction.
Background technique
For example, when manufacturing the other display equipments such as organic EL, liquid crystal display and touch panel, it is main being used to form By in the sputtering of the transparent conductive film constituted such as ITO, IZO, magnetron sputtering becomes mainstream, the magnetron sputtering has been used in circle Mating plates type target on the plate substrate such as plate and the flat pattern sputtering target formed, in addition to this, rotatable sputtering also achieves reality With change, the rotatable sputtering is to make to be bonded to the cylinder type sputtering target of cylinder type target around axis in the outer peripheral surface of cylinder type substrate It rotates and is sputtered.
Moreover, in recent years, with the enlargement of display etc., being also at for the cylinder type sputtering target to its sputtered film Seek the situation of the large-scale sputtering target of the length length of axis direction.
However, just implementing cold isostatic pressing to raw material powder and carrying out heat-agglomerating to it and the circle made of ceramics that makes For cartridge type target, reaches 750mm or more if the length of its axis direction is especially long, thus can generate during fabrication each Kind of problem, therefore the length of cylinder type sputtering target sizing is not easy to.
As the technology for coping with this problem, there is the technology etc. recorded in patent document 1,2.
It describes in patent document 1: for the purpose of the ceramic cylindrical sputtering target material that high density and long size are provided, Before CIP molding, particle is prepared by the slurry containing ceramic material powder and organic additive, relative to ceramic material powder Amount, the amount of organic additive is set as 0.1~1.2 mass %.
Propose in patent document 2: in order to make ceramic cylindrical formed body circumferencial direction it is thickness uniformizing, pass through The method filled ceramic powders in cylindric plug and cylindric framed shaping mould and carry out cold isostatic compaction, makes Shaping mould is pivoted about with the central axis of cylindric plug, while ceramic powders are filled into shaping mould;Using at The fixed funnel in the top of pattern fills ceramic powders into shaping mould.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2013-147368 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2012-139842 bulletin
Summary of the invention
Problem to be solved by the invention
Furthermore when manufacturing the cylinder type target of cylinder type sputtering target of long size as described above, when by cold etc. quiet When compacting (also referred to as CIP) molds cylinder type formed body, warpage archwise can occur in the axial direction for cylinder type formed body Bending.When being ground to cylinder type sintered body obtained from the progress heat-agglomerating of cylinder type formed body, the cylinder type sintered body Outer surface it is smoothened, thus it is as described above bending almost disappear in appearance, therefore it is such bending so far all Not especially as problem.
Here, the previous stock removal in view of eliminating the curved cylinder type sintered body, sets cylinder type formed body, circle The size of cartridge type sintered body, so that the thickness of cylinder type sintered body is greater than defined products thickness in the radial direction.
However, in the case where the cylinder type formed body big to thickness is sintered, because the surface side of thickness direction is in The difference of the temperature changing process of heart side, so that the difference of density and resistance on thickness direction becomes significant.Moreover, sintering Afterwards, it when there is curved cylinder type sintered body its bending to be made to disappear as described above for grinding, is showed in curved influence larger Axis direction end side, stock removal increases, and the part close to thickness direction center exposes as surface.Therefore, manufactured Cylinder type target in, in the end side and center side of axis direction, resistance characteristic is different.As a result, especially in long ruler In very little cylinder type sputtering target, non-uniform resistance characteristic becomes the reason of generating dross, particle on axis direction, in addition also deposits The problem of carrying out difference to the resistance band for being formed by film.
For the present invention to solve the problems, such as this as project of previous cylinder type sputtering target, its purpose is to provide one kind can Inhibit the bending of the cylinder type formed body in the cylinder type target for molding long size and seeks the resistance on axis direction special The cylinder type sputtering target and its manufacturing method of the homogenization of property.
The solution to the problem
Inventor has made intensive studies, and as a result specifies: filling raw material in the forward direction mold for forming of cold isostatic pressing The filling that raw material powder occurs when powder is uneven, since the filling unevenness to suppress generated power in cold isostatic pressing The reason of effect becomes unequal, this is the bending of cylinder type formed body, and it is found that be able to suppress by improving above situation Pass through the bending for the cylinder type formed body that cold isostatic pressing obtains.Thus, it is believed that: the stock removal of cylinder type sintered body can be made to exist Become on axis direction uniformly, can the axis direction of cylinder type target end side and center side by the variation of resistance characteristic Amount inhibits small.
Under the cognition, cylinder type sputtering target of the invention has metal cylinder type substrate and cylinder type made of ceramics Target, the cylinder type target made of ceramics is engaged with the peripheral side of the cylinder type substrate, with the axis direction of 750mm or more Length it is integrally formed, the axis direction of the volume resistivity (bulk resistivity) of the outer peripheral surface of the cylinder type target The coefficient of variation be 0.05 or less.
Here, in cylinder type sputtering target of the invention, it is preferred that the cylinder type target has relative to theoretical density There is 99.0% or more relative density.
In addition, here, in cylinder type sputtering target of the invention, it is preferred that the cylinder type target be ITO, IZO or IGZO。
It should be noted that cylinder type sputtering target of the invention can be the cylinder type substrate and cylinder type target passes through Fusing point is that 200 DEG C of brazing materials below are engaged and formed.
In addition, the manufacturing method of cylinder type sputtering target of the invention is that manufacture has metal cylinder type substrate and ceramics Outside the method for the cylinder type sputtering target of the cylinder type target of system, the cylinder type target made of ceramics and the cylinder type substrate Side engagement, integrally formed with the length of the axis direction of 750mm or more, the manufacturing method includes powder filling work procedure, will Raw material powder fills the cylindric molding space to mold for forming;Molding procedure, after powder filling work procedure, to institute The raw material powder stated in molding space implements cold isostatic pressing, molds cylinder type formed body;And sintering process, in molding work After sequence, to cylinder type formed body carry out heat-agglomerating, obtain cylinder type sintered body, in the powder filling work procedure, at The opening portion of the upper end side in type space configures sieve with covering the opening portion, fills out from the opening portion via sieve to molding space During filling raw material powder, fall the mold for forming to collide striking for the up and down direction in setting face mold for forming application Vibration is hit, the percussion vibration carried out with frequency more than five times for the raw material powder of every 1kg loading, while by raw material powder End filling is to molding space, in the molding procedure, configured with the stiffener from peripheral side bearing mold for forming Under state, cold isostatic pressing is carried out.
It should be noted that the cylinder type can be formed in the manufacturing method of cylinder type sputtering target of the invention The amount of bow of body is set as 1mm or less.
In addition, in the manufacturing method of cylinder type sputtering target of the invention, it can be by the bending of the cylinder type sintered body Amount is set as 4mm or less.
Invention effect
According to the present invention, during fabrication, the filling for being able to suppress the raw material powder in mold for forming is uneven, can prevent The cylinder type formed body obtained by cold isostatic pressing bends.As a result, circle can be equably ground in the axial direction Cartridge type sintered body, it is possible to realize the homogenization of the resistance characteristic on the axis direction of cylinder type sputtering target.
Detailed description of the invention
Fig. 1 is the molding for indicating to can be used in the method for the cylinder type sputtering target of manufacture one embodiment of the present invention Profilograph with mold, including central axis.
Specific embodiment
Hereinafter, detailed description of embodiments of the present invention.
The cylinder type sputtering target of one embodiment of the present invention has metal cylinder type substrate and cylinder made of ceramics Type target, the cylinder type target made of ceramics are engaged via defined brazing material with the peripheral side of cylinder type substrate, with The length of the axis direction of 750mm or more is integrally formed, the axis direction of the volume resistivity of the outer peripheral surface of cylinder type target The coefficient of variation is 0.05 or less.
(composition)
Cylinder type target is target made of ceramics, more specifically, such as is mainly made of ITO, IZO or IGZO.
It is dense by atom comprising indium (In), tin (Sn) and oxygen (O) in the case where cylinder type target is mainly made of ITO (at%) is spent than meter, and Sn/ (In+Sn) is, for example, 0.02~0.40, and typically Sn/ (In+Sn) is 0.02~0.15.
It is dense by atom comprising indium (In), zinc (Zn) and oxygen (O) in the case where cylinder type target is mainly made of IZO (at%) is spent than meter, and Zn/ (In+Zn) is, for example, 0.05~0.25.
It include indium (In), gallium (Ga), zinc (Zn), oxygen (O), example in the case where cylinder type target is mainly made of IGZO Such as, by atomic concentration (at%) than based on, 0.30≤In/ (In+Ga+Zn)≤0.36,0.30≤Ga/ (In+Ga+Zn)≤0.36, 0.30≤Zn/(In+Ga+Zn)≤0.36。
It includes in Fe, Al, Cr, Cu, Ni, Pb, Si that above-mentioned cylinder type target made of ceramics is used as other elements sometimes It is at least one.In this case, total content of these elements is preferably 100 mass ppm or less.When to contain element excessive for these When, worry that membrane property can decline.
The content of above-mentioned Zn, In etc. can be suitably changed according to the electric conductivity etc. of aimed thin film.
The content of In, Zn etc. can be measured by x-ray fluorescence analysis (XRF).
(length of axis direction)
The length of axis direction of the cylinder type target with 750mm or more, throughout the overall length one of the length of its axis direction Body is formed.The cylinder type sputtering target for having the long size of such cylinder type target is promoted in recent years on the display of enlargement There are demands when formation film, and on the other hand, the cylinder type target made of ceramics of the long size is easy to happen bending at the time of molding, Therefore, it is difficult to one is made.In other words, for cylinder type target of the length of axis direction less than 750mm, when forming Bending will not become greater to the variation of resistance characteristic caused by the difference because of the amount of grinding on sintered axis direction and become and ask The degree of topic, there is no need to the application present invention.
On the other hand, when the length of the axis direction of cylinder type target is too long, crackle, bending in sintering process be I'm afraid It can take place frequently.Consider from the viewpoint, in the present invention, cylinder type target for example can be with the length of axis direction for 2000mm or less Target be object.
The length of the axis direction of cylinder type target refers to, by the respective end face of the side of axis direction and the other side The length of the central point line segment connected to each other obtained from shape that is in line.
(volume resistivity)
The coefficient of variation of the axis direction of volume resistivity at the outer peripheral surface of cylinder type target is 0.05 or less.Such as it is logical It crosses and manufactures cylinder type target according to aftermentioned manufacturing method, the coefficient of variation of the axis direction of volume resistivity can be made in this way It is small.
It when the coefficient of variation of the axis direction of volume resistivity is greater than 0.05, has the following problems: becoming and generate particle The reason of, cause film quality to decline in sputtering.
Particle is generated in order to more efficiently prevent from this in sputtering, the coefficient of variation of the axis direction of volume resistivity is excellent 0.05 is selected as hereinafter, more preferably 0.02 or less.The coefficient of variation of the axis direction of volume resistivity is smaller more ideal, therefore not In the presence of the axis direction because of volume resistivity the coefficient of variation it is too small caused by unfavorable condition, but generally 0.005 or more, sometimes It is typically 0.01 or more.
About volume resistivity, with the outer peripheral surface of cylinder type target, that is initially (usually being made for the surface of sputtering The surface of product obtained from outer surface is ground after sintering when making by specified amount) it is object, based on what is recorded in JIS R1637 Four probe method measures the volume resistivity of the outer peripheral surface of cylinder type target.
Moreover, the coefficient of variation of the axis direction about volume resistivity, in the axial direction away from the end of either one 1 point of benchmark is temporarily arranged in the position of 10mm in the circumferential.It 1 lights from this and is measured every 24 ° at total 15 points.With 15 points In, datum mark that point that resistance is minimum is end, be set as being lighted from the benchmark along surface in the straight line that axis direction extends The measurement range of resistance.It is lighted from the benchmark of the end, with 50mm measuring space resistance, until the end 10mm away from opposite side Position.Lighted from the benchmark of end move 90 ° every time clockwise obtained from three straight lines, also carry out same as described above Measurement.Using in each standard deviation on obtained four straight lines, the maximum standard deviation of value as MSD maximum standard deviation, By the MSD maximum standard deviation divided by the average value of all measured values in four straight lines, the axis direction of volume resistivity is calculated The coefficient of variation.That is, the coefficient of variation of the axis direction of volume resistivity passes through the (maximum in each standard deviation of four straight lines Standard deviation)/(average values of all measured values) find out.
(relative density)
The relative density of cylinder type target is preferably 99.0% or more.This is because, in the relative density of cylinder type target In the case where low, it is believed that the reason of this generates electric arc when can become sputtering.
In the present invention, " relative density " is indicated with relative density=(measurement density/theoretical density) × 100 (%).Reason Refer to by density, according to the theoretical density meter of the oxide of the element other than deoxygenation in each constitution element of formed body or sintered body The density value of calculating.For example, if IZO target, then by the oxygen of indium, zinc other than deoxygenation in the indium, zinc, oxygen as each constitution element Compound, that is, indium oxide (In2O3) and zinc oxide (ZnO) be used for theoretical density calculating.Here, by the member of indium and zinc in sintered body Plain assay value (at% or quality %) is converted into indium oxide (In2O3) and zinc oxide (ZnO) mass ratio.For example, for conversion As a result, theoretical density is in the case where the IZO target that indium oxide is 90 mass %, zinc oxide is 10 mass % with { In2O3Density (g/cm3Density (the g/cm of) × 90+ZnO3)×10}/100(g/cm3) calculate.In2O3Density with 7.18g/cm3It calculates, ZnO Density with 5.67g/cm3It calculates, theoretical density is calculated as 7.028 (g/cm3).On the other hand, measurement density refers to that weight is removed To be worth obtained from volume.In the case where sintered body, volume is found out by Archimedes method, then calculate measurement density.
It should be noted that the relative density is so that cylinder type target to be assumed to the mixed of the oxide of contained metallic element The relative density on the basis of theoretical density when conjunction, the true value of the density of the cylinder type target as object tend to than upper The theoretical density stated is high, therefore relative density said here may may also exceed 100% sometimes.
(crystal particle diameter)
The average crystal particle diameter of cylinder type target is preferably 5 μm or less.In the case where average crystal particle diameter is more than 5 μm, Worry that this can become the generating source of particle.Therefore, the average crystal particle diameter of cylinder type target is still more preferably 3 μm or less. Crystal particle diameter is found out according to SEM photograph and using compiling method (code method).About measurement site, in axis direction The sample everywhere that center is along the circumferential direction acquired every 90 ° is object, can be used and is shooting each SEM obtained from these samples All populations and line segment length on the line segment drawn in photo in order to measure calculate average crystal particle diameter.
(brazing material)
Cylinder type sputtering target of the invention is to be bonded to above-mentioned cylinder type in the peripheral side of metal cylinder type substrate Target and formed.
Here, the brazing material engaged between cylinder type substrate and cylinder type target and by them can use fusing point For 200 DEG C of brazing materials below.As such brazing material, as long as can be used for engagement cylinder type substrate and cylinder type The brazing material of target, there is no particular limitation, specifically, In metal, In-Sn metal can be enumerated or be added in In In alloying metal of micro metal component etc..
(manufacturing method)
Above-mentioned have cylinder type target and the cylinder type sputtering target of cylinder type substrate and can for example manufacture as follows.
Firstly, the powder that defined raw material powder is mixed is prepared according to the material of made cylinder type target, It carries out powder filling work procedure: the raw material powder is filled to the cylindric molding space to mold for forming.
As mold for forming, well known mold can be used, such as can be the mould illustrated in Fig. 1 with profilograph Tool.
In the powder filling work procedure, mold for forming 1 is vertically raised as shown in the figure, in this case by raw material powder It puts into from the upper end side of molding space 2 to molding space 2, during filling the raw material powder to molding space 2, is applied with down The percussion vibration in direction, that is, mold for forming 1 is lifted upwards and falls it, every time touches mold for forming 1 Hit its setting face.
According to such case, with the percussion vibration, side is filled to the raw material powder of molding space 2 empty in molding from below Between 2 circumferencial direction equalization stacking, therefore raw material powder molding space 2 circumferencial direction and long dimension direction uniformly to measure Filling.
In particular, here, being set during filling 1kg raw material powder to molding space 2 with frequency hit more than five times Set face, the percussion vibration of Lai Jinhang up and down direction.In the case where the frequency is less than five times, raw material powder is made by percussion vibration It is accumulated in long dimension direction before circumferencial direction homogenization, cannot achieve the uniform filling of raw material powder in end.Therefore, for The raw material powder of every 1kg loading, the frequency that setting face is collided in the percussion vibration of up and down direction are set as more than five times, preferably setting For more than ten times.But even if the frequency is excessively high, it is also unable to reach the homogenization of the filling of this degree or more, therefore the frequency It can be set to 20 times or less.
Moreover, here, for example by using be configured to covering molding space 2 upper end side entire opening portion sieve (not Diagram), the flowing that put into the raw material powder of molding space 2 temporarily ceases at the sieve, and raw material powder is sieved from entire later It equably puts into, therefore raw material powder can be made to fill with uniform amount to molding space 2.The mesh of the sieve can be set to raw material Powder can by size, such as average grain diameter relative to raw material powder is 2~10 times of size.
Then, it carries out molding procedure: the configuration of mold for forming 1 for being filled with raw material powder in molding space 2 is not being schemed In the CIP device shown, cold isostatic pressing is implemented to the raw material powder in molding space 2.Plus-pressure at this time for example can be set to 100MPa~200MPa.
The raw material powder in molding space 2 is pressurizeed around it by compression as a result, can obtain cylinder type formed body.
Here, in powder filling work procedure, as described above, circumferencial direction and long size of the raw material powder in molding space 2 Direction is filled with uniform amount, and filling can be inhibited uneven, thus the plus-pressure of cold isostatic pressing along the circumferential direction with long size side To equably acting on.As a result, can prevent cylinder type formed body from bending.
In molding procedure, as shown in Figure 1, configuration from peripheral side bearing mold for forming 1 stiffener 3 carry out it is cold etc. Static pressure system.Even if stiffener 3 can also be passed through in the case where the length for making axis direction long cylinder type target as a result, It prevents the undesirable bending of the mold for forming 1 when cold isostatic pressing, therefore can more effectively inhibit through above-mentioned behaviour The cylinder type formed body for making to obtain bends.
As long as stiffener 3 supports mold for forming 1 from peripheral side, to bring molding when confrontation cold isostatic pressing to use The component of the curved reinforcement of mold 1, is not particularly limited its shape, for example, it may be in the outer of mold for forming 1 Configure more rod components around cylinder 5 at a prescribed interval each other.
Implementing cylinder type formed body obtained from cold isostatic pressing to raw material powder so in molding procedure, preferably its is curved Song amount is 1mm or less.In the case where the amount of bow of cylinder type formed body is more than 1mm, in aftermentioned sintered grinding, it is Bending is set to disappear, it has to substantially change stock removal in the axial direction, therefore worry the body of the outer peripheral surface of cylinder type target Product resistivity becomes uneven in the axial direction.Therefore, the amount of bow of cylinder type formed body be still more preferably 0.5mm with Under.
The amount of bow of the cylinder type formed body using ruler (straight edge) and feeler gauge (feeler gauge) into Row measurement.Amount of bow about aftermentioned cylinder type sintered body is also same.
After the forming step, it is sintered process: the cylinder of size will be had adjusted as desired by lathe process etc. The setting of type formed body is placed on setting face, i.e., configures according to the central axis direction vertical with setting face, in this case, such as 1300 DEG C~1600 DEG C at a temperature of carry out heat-agglomerating in 20 hours~200 hours, obtain cylinder type sintered body.
By the heat-agglomerating in sintering process, the difference of sintering sequence due to caused by the heated condition of furnace is shunk The difference etc. of behavior, the amount of bow of usual cylinder type sintered body are greater than the amount of bow of cylinder type formed body.In this manufacturing method, It, can due to the bending of the mold for forming 1 when preventing the filling of raw material powder uneven, cold isostatic pressing as described above Reduce the amount of bow of cylinder type sintered body.Specifically, the amount of bow of cylinder type sintered body is preferably 4mm or less.Work as cylinder type When the amount of bow of sintered body is more than 4mm, when being ground the outer surface of cylinder type sintered body, it is sometimes desirable to make stock removal in axis side Differ widely upwards, probably will lead to the variation of the axis direction of the volume resistivity of the outer peripheral surface of cylinder type target as a result, Increase.
Later, the outer surface of cylinder type sintered body, production are ground by method well known to mechanical grinding or chemical grinding etc. Cylinder type target.The grinding is preferably on the basis of the thickness direction of cylinder type sintered body, the face for being zero by amount of bow, then is ground 0.1mm or more.
The obtained cylinder type target is configured in the peripheral side of metal cylinder type substrate, is made molten as described above Point is that 200 DEG C of brazing materials below etc. are flowed between cylinder type target and cylinder type substrate with molten condition, is made by cooling It solidifies, and cylinder type target and cylinder type substrate are interconnected using the brazing material.
Thereby, it is possible to manufacture cylinder type sputtering target.
Embodiment
Then, sputtering target of the invention is manufactured experimently, it is thus identified that its performance, it is described below.But explanation here is In order to illustrate, it is not intended to be defined in this.
The raw material powder that ratio by indium oxide powder and tin oxide with weight ratio for 90:10 mixes is filled to molding and is used The molding space of mold implements the cold isostatic pressing under the plus-pressure of 30 minutes 150MPa to it, obtains cylinder type formed body. The cylinder type formed body is heated to 1500 DEG C of temperature in furnace, is kept for 50 hours to be sintered, cooled down later.It is right Thus obtained cylinder type sintered body cuts 0.1mm by regrinding on the basis of being machined the face for being zero by amount of bow, and production is provided There are the Examples 1 to 4 of the length of axis direction shown in table 1 and the cylinder type target of the Comparative Examples 1 to 5.
[table 1]
In embodiment 1, when powder is filled, the sieve of 2~10 times of mesh of the average grain diameter of raw material powder has been used The filling for carrying out raw material powder carries out ten percussion vibrations for every 1kg loading, and at the time of molding using as shown in Figure 1 Plurality of rods shape stiffener carried out the reinforcement of mold for forming.In embodiment 2~4, change cylinder as shown in table 1 respectively The length of the axis direction of type target, makes similarly to Example 1 in addition to this.
In comparative example 1, raw material filling is not carried out using sieve, is made similarly to Example 1 in addition to this.Comparing In example 2, percussion vibration is not carried out, is made similarly to Example 2 in addition to this.In comparative example 3, when not carrying out CIP Reinforcement, make similarly to Example 3 in addition to this.
In comparative example 4, percussion vibration makes similarly to Example 4 in addition to this less than five times.In comparative example 5, In the raw material filling carried out using sieve, mesh has been used to be greater than 10 times of sieve of the average grain diameter of raw material powder, in addition to this It makes similarly to Example 1.
It should be noted that " 〇 " of the mesh of sieve refers in table 1, mesh is the 10 of the average grain diameter of raw material powder Again hereinafter, " △ " refers to, mesh is greater than 10 times of the average grain diameter of raw material powder, and "×" refers to, not using sieve.In addition, striking " 〇 " for hitting number refers to, carries out percussion vibration more than five times for every 1kg loading, " △ " refers to, every 1kg is filled Amount carries out the percussion vibration less than five times, and "×" refers to, does not carry out percussion vibration.In addition, " 〇 " of reinforcement when CIP is Refer to, used stiffener, "×" refers to, does not use stiffener.
The ratio of the average grain diameter of mesh size and raw material powder for sieve, the average grain diameter of raw material powder in each example Sometimes also slightly different, therefore be not strict with, but substantially, it the use of mesh is average grain diameter in the case where " 〇 " of table 1 Three kinds of 2~5 times, 5~8 times and 8~10 times or so sieves, in the case where " △ ", using mesh is the 11 of average grain diameter A kind of~15 times or so of sieve.
About the above embodiments 1~4 and the Comparative Examples 1 to 5, cylinder type formed body and cylinder are determined by the above method The respective amount of bow of type sintered body, the results are shown in Table 1.
In the Comparative Examples 1 to 5, compared with Examples 1 to 4, the bending of sintered body becomes larger.Especially with regard to comparative example 4, Number of taps be twice, four times when, can not effectively inhibit the bending of sintered body.In addition, using mesh mistake about comparative example 5 When big sieve, the curved inhibition of sintered body is insufficient.
In addition, each cylinder type target about Examples 1 to 4 and the Comparative Examples 1 to 5, is surveyed using the resistivity of NPS corporation The volume resistivity for determining device (model: Σ 5+) measurement outer peripheral surface, finds out the coefficient of variation of the axis direction of the volume resistivity.Its As a result it is also depicted in table 1.
Make the peripheral side of the cylinder type target of Examples 1 to 4 and the Comparative Examples 1 to 5 Yu cylinder type substrate via brazing material Engagement, using it in investment electric power 4.0kW/m, Ar throughput: being sputtered under conditions of 20Sccm, sputtering time 24 hours. As a result, on the basis of by the granule number of embodiment 1, when the granule number of embodiment 1 is set as 100, of embodiment 2~4 Grain number is 150 hereinafter, the granule number of comparative example is 500~900.
It should be noted that the cylinder type target about IZO and IGZO, also with said circumstances substantially in the same manner as manufacture experimently simultaneously Tested, as a result, obtained it is almost same as a result, it can thus be appreciated that: according to the present invention, ITO, IZO and IGZO In any cylinder type target be able to suppress the bending of formed body, sintered body, can be realized the resistance characteristic of axis direction Homogenization.
Description of symbols
1: mold for forming;2: molding space;3: stiffener.

Claims (7)

1. a kind of cylinder type sputtering target has metal cylinder type substrate and cylinder type target made of ceramics, the ceramics The cylinder type target of system is engaged with the peripheral side of the cylinder type substrate, with one bodily form of length of the axis direction of 750mm or more At the coefficient of variation of the axis direction of the volume resistivity of the outer peripheral surface of the cylinder type target is 0.05 or less.
2. cylinder type sputtering target according to claim 1, wherein
The cylinder type target has 99.0% or more relative density relative to theoretical density.
3. cylinder type sputtering target according to claim 1 or 2, wherein
The cylinder type target is ITO, IZO or IGZO.
4. cylinder type sputtering target described in any one of claim 1 to 3, wherein
The cylinder type sputtering target is that the cylinder type substrate and cylinder type target pass through fusing point as 200 DEG C of brazing materials below Engagement and formed.
5. a kind of manufacturing method of cylinder type sputtering target is that manufacture has metal cylinder type substrate and cylinder made of ceramics The periphery of the method for the cylinder type sputtering target of type target, the cylinder type target made of ceramics and the cylinder type substrate flanks It closes, it is integrally formed with the length of the axis direction of 750mm or more,
The manufacturing method includes
Raw material powder is filled the cylindric molding space to mold for forming by powder filling work procedure;
Molding procedure implements cold isostatic pressing, molding to the raw material powder in the molding space after powder filling work procedure Cylinder type formed body out;And
Sintering process carries out heat-agglomerating to cylinder type formed body, obtains cylinder type sintered body after the forming step,
In the powder filling work procedure, in the opening portion of the upper end side of molding space, configure sieve with covering the opening portion, from During raw material powder is filled to molding space via sieve in the opening portion, fall the mold for forming mold for forming application Under to collide the percussion vibration of the up and down direction in setting face, for every 1kg loading raw material powder with frequency more than five times The percussion vibration is carried out, while raw material powder being filled to molding space, in the molding procedure, is being configured with from periphery In the state of the stiffener of side bearing mold for forming, cold isostatic pressing is carried out.
6. the manufacturing method of cylinder type sputtering target according to claim 5, wherein
The amount of bow of the cylinder type formed body is 1mm or less.
7. the manufacturing method of cylinder type sputtering target according to claim 5 or 6, wherein
The amount of bow of the cylinder type sintered body is 4mm or less.
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